Experiment 7 potentiometric titration
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Experiment 7 Potentiometric Titration. Valdosta State University. Purpose. To accurately determine the molar mass and pK a of an unknown weak acid. Valdosta State University. Background. In this experiment, the pH of a solution will be measured directly as the sodium hydroxide is added.

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Experiment 7 Potentiometric Titration

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Experiment 7 potentiometric titration

Experiment 7Potentiometric Titration

Valdosta State University


Purpose

Purpose

To accurately determine the molar mass and pKa of an unknown weak acid.

Valdosta State University


Background

Background

  • In this experiment, the pH of a solution will be measured directly as the sodium hydroxide is added.

  • The pH will be measured using a glass combination electrode.

  • This device measures pH (or [H3O+]) as voltage.

Valdosta State University


Background1

Background

  • pH Combination Electrode

    • combination refers to the ion sensing cell and the reference cell.

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Background2

Background

  • pH Combination Electrode

    • combination refers to the ion sensing cell and the reference cell.

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Background3

Background

Consider the following graph:

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Background4

Background

Consider the following graph:

In this region H+ dominates, the small change in pH is the result of relatively small changes in H+ concentration.

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Background5

Background

Consider the following graph:

In this region, relatively small changes in H+ concentration cause large changes in pH, The midpoint of the vertical region is the equivalence point.

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Background6

Background

Consider the following graph:

In this region OH- dominates, the small change in pH is the result of relatively small changes in OH- concentration.

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Background7

Background

HA(aq) + NaOH(aq)  NaA(aq) + H2O(l)

  • This experiment will use monoprotic acids.

  • Therefore, at the equivalence point,moles HA = moles NaOH

  • Using the definition of moles, the molar mass can be determined:

Valdosta State University


Background8

Background

HA(aq) + NaOH(aq)  NaA(aq) + H2O(l)

  • This experiment will use monoprotic acids.

  • Therefore, at the equivalence point,moles HA = moles NaOH

  • Using the definition of moles, the molar mass can be determined:

Valdosta State University


Background9

Background

HA(aq) + NaOH(aq)  NaA(aq) + H2O(l)

  • pKa can be determined by using the Henderson-Hasselbach equation.

Valdosta State University


Background10

Background

HA(aq) + NaOH(aq)  NaA(aq) + H2O(l)

  • pKa can be determined by using the Henderson-Hasselbach equation.

Valdosta State University


Background11

Background

HA(aq) + NaOH(aq)  NaA(aq) + H2O(l)

  • pKa can be determined by using the Henderson-Hasselbach equation.

  • If the pH is measured at the point where[conjugate base] = [weak acid]

Valdosta State University


Background12

Background

HA(aq) + NaOH(aq)  NaA(aq) + H2O(l)

  • pKa can be determined by using the Henderson-Hasselbach equation.

  • If the pH is measured at the point where [conjugate base] = [weak acid]

Valdosta State University


Background13

Background

HA(aq) + NaOH(aq)  NaA(aq) + H2O(l)

  • This assumption is valid at the half-titration point.

  • If the equivalence point is 20.00mL, the half-titration point is at 10.00mL.

  • The pH is then obtained directly from the graph.

Valdosta State University


Background14

Background

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Background15

Background

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Background16

Background

5.2

9.1mL

18.2mL

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Procedure experiment 7

Procedure – Experiment 7

- For this experiment, work in pairs.


Technique titration

Technique - Titration

  • Clean The Buret

  • Rinse a buret twice with distilled water.

  • Rinse the buret twice with 10-mL portions of your standardized NaOH solution.

  • Run some of the NaOH solution through the tip of the buret.

  • Drain the buret, then fill it with the standardized NaOH solution.

  • Let some NaOH solution run through the tip of the buret so that all air bubbles are removed.


Technique titration1

Technique - Titration

Clean The Buret


Technique titration2

Technique - Titration

  • Prepare the Unknown

  • Weigh 0.300 – 0.400g of solid unknown or 0.120 – 0.180g of liquid unknown to the nearest 0.001 g into a 250mL beaker.

  • Add approximately 50 mL of distilled water to the beaker and stir until all the unknown is dissolved.


Technique titration3

Technique - Titration

Set-up the pH electrode – GLX Computer


Technique titration4

Technique - Titration

  • Set-up the pH meter - Calibration

  • Get a 400 mL beaker of distilled water to rinse the electrode between readings. Rinse the electrode with distilled water.


Technique titration5

Technique - Titration

  • Performing The Experiment

  • Put the electrode tip in the unknown acid solution. “Start” button on

  • Fill the buret to 0.00mL and record this initial pH and buret reading.

  • Slowly add NaOH with stirring until either the pH increases by 0.20 units or 2.0 mL of NaOH have been added, whichever occurs first. Stop and record both the pH and the buret reading.

  • Repeat step 3 until the pH reaches 12, or until the titration has gone 15 mL past the equivalence point.


Experiment 7 potentiometric titration

Data

Mass of unknown: 0.449g


Experiment 7 potentiometric titration

Data


Experiment 7 potentiometric titration

Data

18.5 mL


Calculation molar mass

Calculation – Molar Mass


Calculation molar mass1

Calculation – Molar Mass


Calculation molar mass2

Calculation – Molar Mass


Calculation pk a

Calculation - pKa

9.25 mL

18.5 mL


Calculation pk a1

Calculation - pKa

5.08

9.25 mL

18.5 mL


Important reminder

IMPORTANT REMINDER

Save the unused solution in a location identified by your laboratory instructor.

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Safety

Safety

The NaOH solutions are corrosive. If you get some on your skin, wash with water for at least five minutes. If any NaOH solution gets in the eyes IMMEDIATELY wash with water for at least fifteen minutes. Call for medical assistance!

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Waste disposal

Waste Disposal

All wastes from this experiment can be flushed down the drain with plenty of running water.

Valdosta State University


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